1,4-Bis(tert-butoxycarbonyl)-2-[3-(thien-2-yl)-2-propenyl]piperazine → 1,4-Bis(tert-butoxycarbonyl)-2-[3-(thien-2-yl)propyl]piperazine

HRID 352833ノート

反応式

HRID 352833 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH:9]1[CH2:21][CH:22]=[CH:23][C:24]1[S:25][CH:26]=[CH:27][CH:28]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>CO.[C].[Pd]>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:18])([CH3:19])[CH3:20])=[O:15])[CH2:10][CH:9]1[CH2:21][CH2:22][CH2:23][C:24]1[S:25][CH:26]=[CH:27][CH:28]=1)=[O:7])([CH3:2])([CH3:3])[CH3:4]

参加物

4

反応物 1

HCID 698800971,4-Bis(tert-butoxycarbonyl)-2-[3-(thien-2-yl)-2-propenyl]piperazine

生成物 1

HCID 227104421,4-Bis(tert-butoxycarbonyl)-2-[3-(thien-2-yl)propyl]piperazine

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

In methanol (70 ml) was dissolved 1,4-bis(tert-butoxycarbonyl)-2-[3-(thien-2-yl)-2-propenyl]piperazine (1.01 g). In the resulting solution was suspended 10% palladium-carbon (50% wet, 431 mg), followed by vigorous shaking at room temperature for 6 hours under a hydrogen gas atmosphere of 1 atmospheric pressure. The catalyst was filtered off and the filtrate was concentrated under reduced pressure. The residue was subjected to chromatography on a silica gel column (hexane:ethyl acetate=9:1 to 2:1), whereby the title compound (975 mg) was obtained as colorless powder.

後処理

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customwas obtained as colorless powder

出典と根拠

ORDレコード
ord-bfbc531641b94f088bb8f58effd1d466
出典データセット
uspto-grants-2004_06
特許番号
US06747023B1

反応ノート

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